CN106076336A - A kind of preparation method of magnetic ferric oxide nano piece - Google Patents
A kind of preparation method of magnetic ferric oxide nano piece Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims abstract description 8
- 229940001447 lactate Drugs 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims abstract description 6
- 239000008156 Ringer's lactate solution Substances 0.000 claims abstract description 6
- 238000002242 deionisation method Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 239000012855 volatile organic compound Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229960001545 hydrotalcite Drugs 0.000 description 3
- 229910001701 hydrotalcite Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- GJYCVCVHRSWLNY-UHFFFAOYSA-N 2-butylphenol Chemical compound CCCCC1=CC=CC=C1O GJYCVCVHRSWLNY-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IHICGCFKGWYHSF-UHFFFAOYSA-N C1=CC=CC=C1.CC1=CC=CC=C1.CC1=CC=CC=C1C Chemical compound C1=CC=CC=C1.CC1=CC=CC=C1.CC1=CC=CC=C1C IHICGCFKGWYHSF-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
- B01D2253/1124—Metal oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Power Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention discloses the preparation method of a kind of magnetic ferric oxide nano piece.In turn include the following steps: take 500mL FeCl2Solution, it is placed in 70~80 DEG C of water-baths of constant temperature, in solution, is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH weak solution, keep pH value to be 12~13, reaction 2~3h, proceed in autoclave, in 1h, be warmed up to 150~180 DEG C, continue reaction 4~8h, naturally cool to room temperature, forming the precipitation with layer structure, precipitate and separate in this process, deionization is washed 2~3 times;The solid obtaining precipitation joins in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio is 1:10~1:50, stirring 4~5h, precipitate and separate, the solid obtaining is after being washed with deionized 2~3 times, calcine at a temperature of 400~450 DEG C, remove lactate therein, i.e. can get a kind of ferric oxide nano piece.This structure is conducive to absorption and catalysis pollutant, is conducive to separating simultaneously.
Description
Technical field
The present invention relates to the exploitation of novel environmental pollution control material, particularly relate to the preparation side of a kind of ferric oxide nano piece
Method.
Background technology
VOCs treatment refers to that the organic exhaust gas producing in industrial processes carries out the place adsorbed, filter, purify
Science and engineering is made.Usual VOCs treatment has the benzene homologues VOCs treatment such as formaldehyde VOCs treatment, benzene toluene dimethylbenzene etc.
Deng.Organic exhaust gas be usually present inflammable and explosive, poisonous and harmful, water insoluble, be dissolved in the big spy of organic solvent, intractability
Point.Commonly used when VOCs treatment is organic exhaust gas active-carbon adsorption treatment method, Production by Catalytic Combustion Process, catalysis oxidation
Multiple principles such as method, acid-base neutralization method, plasma method.Catalysis oxidation is a kind of both economical effective method.But need through
Ji is suitable for blanket catalyst.
Nano-sized iron oxide has good weatherability, light resistance, magnetic and has good absorption and shielding to ultraviolet
Effect, is a kind of important inorganic material.Have important in fields such as catalysis, function ceramics, magnetic material and transparent pigments
Application.Nano-sized iron oxide has huge specific surface area, and skin effect is notable, is also a kind of good catalyst.Use nanoparticle
The activity of the catalyst that son is made, selectivity are all higher than typical catalyst, and life-span length easily operates.To make of nano-sized iron oxide
The hollow beads becoming, floats on the wastewater surface containing organic matter.The degraded utilizing sunshine to carry out organic matter can be accelerated at waste water
Reason process.Nano-sized iron oxide has been directly used as the catalyst of high molecular polymer oxidation, reduction and synthesis, butylphenol Catalyzed by Nano-ferric Oxide
Agent can make the rate of cleavage of oil improve 1~5 times, using the burning velocity of its solid propellant made as combustion catalyst relatively
Conventional propellant can improve 1~10 times, and this is highly beneficial to manufacture high-performance rocket and guided missile.Nano-sized iron oxide can also be catalyzed
Decomposition water, makes clean energy resource.
Made magnetic nanometer composite material can effectively prevent nanometer by magnetic nanoparticle being dispersed in certain matrix
Intergranular mutual reunion, efficiently controls its particle size.To lead additionally, magnetic-particle is embedded in immiscible medium
Cause some unusual Physical and chemical characteristics.
Hydrotalcite-based compound (LDHs) is the compound piled up by interlayer anion and positively charged laminate.Neatly
Stone chemical structure of general formula is: [M2+ 1-xM3+x(OH)2]x+[(An-)x/n·mH2O], wherein M2+And M3+It is respectively positioned at main body laminate
On divalence and trivalent metal cation, such as Mg2+、Ni2+、Zn2+、Mn2+、Cu2+、Co2+、Pd2+、Fe2+Deng bivalent cation and Al3 +、Cr3+、Co3+、Fe3+All can form hydrotalcite Deng Tricationic;An–For interlayer anion, inorganic anion can be included,
Organic anion, complex anion, same many and heteropolyanion;X is M3+/(M2++M3+) molar ratio, about 4:1 arrives
2:1;M is the number of intermediary water molecule.It is similar to that shepardite Mg (OH)2, octahedron is shared seamed edge and forms main body
Laminate.The divalent metal M being positioned on laminate2+Can be golden by the close trivalent of ion half price in certain proportion
Belong to cation M3+Same order elements so that laminate is positively charged, interlayer exist can exchange anion and laminate on positive electricity
Lotus balances so that the overall structure of LDHs is electroneutral.The anion of interlayer can be exchanged, through a series of modifications, hydrotalcite
Material can obtain many materials planting different properties.
Content of the invention
It is an object of the invention to, for overcoming the deficiency that iron oxide structure in prior art is single, provide a kind of ferric oxide nano
The preparation method of piece.
The technical solution used in the present invention is in turn include the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2~3mol/L, take this solution of 500mL, Xiang Qi
In be placed in 70~80 DEG C of water-baths of constant temperature, be simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH dilute molten
Liquid, keeps pH value to be 12~13, reacts 2~3h, proceed in autoclave, be warmed up to 150~180 DEG C in 1h, continue reaction 4~
8h, naturally cools to room temperature, forms the precipitation with layer structure, precipitate and separate in this process, and deionization is washed 2~3 times;
2) solid that precipitation obtains is joined in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio be 1:10~
1:50, stir 4~5h, precipitate and separate, it is thus achieved that solid after being washed with deionized 2~3 times, the temperature of 400~450 DEG C
The lower calcining of degree, removes lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
The invention have the advantage that the ferric iron that part ferrous ion is generated by hydrogen peroxide oxidation, divalent ion and generation
Trivalent ion alkali in 70~80 DEG C of water-baths effect under, produce magnetic co-precipitation, form lamella hydrotalcite structure, then at piece
Inter layer exchange enters lactate, removes lactate finally by high-temperature calcination, forms the lamellar structure relatively scattered.This structure has
It is beneficial to absorption and catalysis pollutant.
Detailed description of the invention
3 embodiments of the offer present invention further below:
Embodiment 1
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, be placed in wherein
In 80 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 4mL and a certain amount of NaOH weak solution, holding pH value is
13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 8h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times;The solid obtaining precipitation joins concentration
In the sodium lactate solution of 4mol/L, solid-to-liquid ratio is 1:50, stir 5h, precipitate and separate, it is thus achieved that solid be washed with deionized 3
All over afterwards, calcine at a temperature of 450 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality
Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 97.2%, supernatant can be arranged
Put.
Embodiment 2
By FeCl2It is dissolved in water, is configured to the solution that concentration is 2mol/L, take this solution of 500mL, be placed in wherein
In 70 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2mL and a certain amount of NaOH weak solution, holding pH value is
12, react 2h, proceed in autoclave, in 1h, be warmed up to 150 DEG C, continue reaction 4h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 2 times;The solid obtaining precipitation joins concentration
In the sodium lactate solution of 2mol/L, solid-to-liquid ratio is 1:10, stir 4h, precipitate and separate, it is thus achieved that solid be washed with deionized 2
All over afterwards, calcine at a temperature of 400 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality
Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 97.5%, supernatant can be arranged
Put.
Embodiment 3
By FeCl2It is dissolved in water, is configured to the solution that concentration is 3mol/L, take this solution of 500mL, be placed in wherein
In 80 DEG C of water-baths of constant temperature, being simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 3mL and a certain amount of NaOH weak solution, holding pH value is
13, react 3h, proceed in autoclave, in 1h, be warmed up to 180 DEG C, continue reaction 6h, naturally cool to room temperature, in this process
Forming the precipitation with layer structure, precipitate and separate, deionization is washed 3 times;The solid obtaining precipitation joins concentration
In the sodium lactate solution of 4mol/L, solid-to-liquid ratio is 1:50, stir 5h, precipitate and separate, it is thus achieved that solid be washed with deionized 3
All over afterwards, calcine at a temperature of 450 DEG C, remove lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
Take 1g ferric oxide nano piece, join in the pending methylene blue waste water of 1.0L, add 0.01 milliliter of quality
Fraction is the hydrogen peroxide of 30%, stirs 20min, and organic matter is decomposed, and magnetic field separates, and clearance 94.3%, supernatant can be arranged
Put.
Claims (1)
1. a preparation method for magnetic ferric oxide nano piece, is characterized in that in turn including the following steps:
1) by FeCl2It is dissolved in water, is configured to the solution that concentration is 2~3mol/L, take this solution of 500mL, be placed in wherein
It in 70~80 DEG C of water-baths of constant temperature, is simultaneously added dropwise 30% (mass fraction) hydrogen peroxide 2~4mL and a certain amount of NaOH weak solution, protect
Holding pH value is 12~13, reacts 2~3h, proceeds in autoclave, be warmed up to 150~180 DEG C in 1h, continues reaction 4~8h, from
So being cooled to room temperature, forming the precipitation with layer structure, precipitate and separate in this process, deionization is washed 2~3 times;
2) joining the solid that precipitation obtains in the sodium lactate solution that concentration is 2~4mol/L, solid-to-liquid ratio is 1:10~1:50,
Stirring 4~5h, precipitate and separate, it is thus achieved that solid after being washed with deionized 2~3 times, at a temperature of 400~450 DEG C
Calcining, removes lactate therein, i.e. can get a kind of magnetic ferric oxide nano piece.
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Cited By (2)
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CN107899578A (en) * | 2017-10-25 | 2018-04-13 | 浙江科技学院 | A kind of heterogeneous class light fenton catalyst of rice-pudding shape micron ferric oxide and preparation method thereof |
CN108186677A (en) * | 2018-01-05 | 2018-06-22 | 中国科学院上海硅酸盐研究所 | Degradable nano material that new free-radical efficiently generates and its preparation method and application |
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2016
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107899578A (en) * | 2017-10-25 | 2018-04-13 | 浙江科技学院 | A kind of heterogeneous class light fenton catalyst of rice-pudding shape micron ferric oxide and preparation method thereof |
CN107899578B (en) * | 2017-10-25 | 2020-05-26 | 浙江科技学院 | Zongzi-shaped micron-sized iron oxide heterogeneous photo-Fenton catalyst and preparation method thereof |
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CN108186677B (en) * | 2018-01-05 | 2020-05-19 | 中国科学院上海硅酸盐研究所 | Degradable nano material capable of efficiently generating free radicals and preparation method and application thereof |
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